CN103866175A - Ferrous vanadium nitride (FeV65N13) and synthetic method thereof - Google Patents
Ferrous vanadium nitride (FeV65N13) and synthetic method thereof Download PDFInfo
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- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title abstract description 8
- 238000010189 synthetic method Methods 0.000 title abstract description 5
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title abstract 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 83
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 44
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920002994 synthetic fiber Polymers 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 4
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 claims description 76
- 229910000628 Ferrovanadium Inorganic materials 0.000 claims description 34
- -1 ferrovanadium nitride Chemical class 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 29
- 229910000831 Steel Inorganic materials 0.000 claims description 22
- 239000010959 steel Substances 0.000 claims description 22
- 230000015572 biosynthetic process Effects 0.000 claims description 12
- 238000003786 synthesis reaction Methods 0.000 claims description 12
- 238000005049 combustion synthesis Methods 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
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- 238000001816 cooling Methods 0.000 claims description 4
- 229910000756 V alloy Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 2
- 229910001208 Crucible steel Inorganic materials 0.000 claims description 2
- 229910001315 Tool steel Inorganic materials 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 2
- 240000003936 Plumbago auriculata Species 0.000 claims 1
- 239000013589 supplement Substances 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 34
- 238000002485 combustion reaction Methods 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 3
- 229910002804 graphite Inorganic materials 0.000 abstract 2
- 238000004519 manufacturing process Methods 0.000 description 33
- 229910045601 alloy Inorganic materials 0.000 description 16
- 239000000956 alloy Substances 0.000 description 16
- 235000019580 granularity Nutrition 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 10
- 239000003701 inert diluent Substances 0.000 description 9
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 9
- 238000005275 alloying Methods 0.000 description 7
- 230000003014 reinforcing effect Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 229910001021 Ferroalloy Inorganic materials 0.000 description 5
- 241000209456 Plumbago Species 0.000 description 5
- 229910001294 Reinforcing steel Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 229910001566 austenite Inorganic materials 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
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- 229910000859 α-Fe Inorganic materials 0.000 description 3
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
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- 238000007789 sealing Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
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- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000742 Microalloyed steel Inorganic materials 0.000 description 1
- 229910001199 N alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
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- 230000007774 longterm Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 230000001902 propagating effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- 229910052719 titanium Inorganic materials 0.000 description 1
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- 238000013519 translation Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Treatment Of Steel In Its Molten State (AREA)
Abstract
The invention provides a ferrous vanadium nitride (FeV65N13) and a synthetic method thereof. The ferrous vanadium nitride is composed of 63.0-67.0% of V, 12.0-16.0% of N and the balance of iron and few impurities in percentage by mass. The raw materials adopted include ferrous vanadium 80 (FeV80) and ferrous vanadium 50 (FeV50). A ferrous vanadium synthetic material powder is evenly mixed and then put in a graphite crucible in bulk, next, the graphite crucible is put in a high-pressure synthetic furnace, the amount of nitrogen needed is calculated according to the vanadium content of the synthetic material, high-purity nitrogen with the pressure of 7 to 12MPa is charged and ignited by using an ignition device to carry out a synthetic reaction, the pressure is maintained by introducing the high-purity nitrogen again when the nitrogen pressure is reduced to 6.5MPa until the combustion synthetic reaction is completed continuously, and no external heat energy needs to be supplied in the reaction, and furthermore, the combustion synthetic product is cooled in nitrogen and crushed into lumpiness required by a user after being discharged from a furnace.
Description
Technical field
The invention belongs to the production method of the nitrogenous iron alloy of burning synthetic (being called for short CS) (also claim self propagating high temperature synthetic, be called for short SHS), be specifically mainly applicable to the production method of FeV65N13 ferrovanadium nitride product.
Background technology
Along with the fast development of world today's building industry and reinforcing bar production technology, the engineering structures such as Infrastructure, Highrise buildings are more and more higher to the requirement of reinforcement property.High strength is the important development direction of concrete reinforcement.It is reported, the reinforcing bar employing rate of Britain, Australia, Japan and other countries 400MPa reaches 80～90%; In Germany, concrete construction has all been upgraded to IV grade reinforcing steel taking 500MPa as main with reinforcing bar, and Japan has developed the superstrength reinforcing bar that yield strength is 685～980MPa, and for Highrise buildings.China is through each side's effort in recent years, and the consumption of the III grade reinforcing steel of 400MPa accounts for 50% left and right, has obtained huge progress, but still there is a big difference with advanced international standard.
The III grade reinforcing steel of promoting the use of 400MPa is the requirement of China's relevant policies, house and town and country construction portion, the Ministry of Industry and Information Technology combined and have put into effect " about industry restructuring guidance list (basis in 2011) " on January 16th, 2012, relevant clause determines, HRB335 grade reinforcing steel is classified as to obsolete product, and this clause is implemented on May 1st, 2013.Catching the environment opportunity of market and technological standard, expand the application percentage of III level, IV grade reinforcing steel, promote the upgrading of China's reinforcing bar quality, is nearly 5 years of Chinese architecture reinforcing bar field and even long-term task.
Micro-alloying technology is in the utilization in Iron And Steel Industry field, and to present steel industrial technology, progress has played very large prograding.Microalloying refers to and on the basis of former alloy, adds the carboritride forming elements such as micro-niobium, vanadium, titanium again, and its add-on is generally 0.02-0.20%.Separating out with refinement ferrite crystal grain by microalloy element carboritride in steel makes steel reach high strength, thereby embodies the economic advantages of micro-alloying technology, and micro-alloying technology is widely used in the production of High Strength Steel at present.In three micro alloying elements, vanadium is effective and the most the most frequently used micro alloying element.China is vanadium resource big country, and reserves are abundant, and vanadium goods output occupies third place in the world, therefore in resource, has advantage in China's development Vanadium Microalloyed Plate Steels.
The eighties in 20th century, according to recrystallize controlled rolling theory, develop the Hi-Stren steel of a series of employing Vanadium Microalloyed Plate Steels, and obtained application widely.In production technique, the feature of Vanadium Microalloyed Plate Steels is to adopt the higher austenite recrystallization district controlled rolling of temperature, it has overcome the restriction containing conditions such as niobium steel must adopt low temperature, heavy reduction rate, large rolling load and treat that the temperature residence time is grown, improve production efficiency, improved economy.Vanadium Microalloyed Plate Steels is best suited for the production that accounts for more than 50% long profiles of steel ultimate production.Vanadium in Vanadium Microalloyed Plate Steels, by forming vanadium nitride, by the harmful element nitrogen in steel, transform favourable cheap alloying element as.Under the cooperation of nitrogen, the carbonitride of vanadium not only can be separated out at high temperature austenite, stops Austenite Grain Growth, increases phase transformation core, and can separate out in the lower ferrite area of temperature, increases the ferritic raw nuclear location of intracrystalline, refinement ferrite crystal grain.
The U.S. is the country of studying the earliest VN alloy, just discloses relevant patent US3334992 as far back as 1967, subsequently at 1968,1977 and 1985 reports that have a United States Patent (USP).South Africa Vametco mining company of American strategy mineral company, after within 1986, setting up, provides to the travelling trader of countries in the world the vanadium and the related products that exceed 9000 tons every year.Its vanadium nitrogen product grade is Nitrovan7, Nitrovan12, Nitrovan16, wherein Nitrovan12 consumption maximum.At home, " 95 " brainstorm project was listed in the research and development of VN alloy in, and built up the commerical test line of producing 300 tons per year in 2002, and enlarging in 2003 is 1000 tons of VN alloy industrialization production lines, and its production technology principle is similar to the technique of the U.S..
1998, year American strategy mineral companies (Ji Fan company) start technological cooperation with Iron and Steel Research Geueral Inst, carry out the exploitation of V-n Microalloying Technology and applying of vanadium-nitrogen alloy product thereof at Chinese steel industry.Domestic each research unit and large steel mill have carried out a large amount of tests to the VN alloy of the U.S..And to adding in steel after cheap nitrogen alloying element, the mechanical property to steel and strengthening mechanism have been carried out deep discussion.Especially in the production practice of producing III level Twisted Steel, carried out application widely, V-N reinforcing bar is under same intensity level, and the addition of vanadium reduces by 50% left and right.VN alloy has become the important source material of producing III level Twisted Steel and Vanadium Microalloyed Plate Steels.
From 2003 the inventor to adopt commodity vanadium iron be raw material, study the production technique of ferrovanadium nitride by the synthetic hi-tech of burning, and set up a trial production line with independent intellectual property right thereupon.Due to business vanadium iron raw material ingredient stability and high pressure nitriding complete, therefore product composition is highly stable.Ferrovanadium nitride product at home some large steel mills carries out the production and application of III level Twisted Steel and part V-N microalloyed steel, result on trial shows, its result of use is identical with VN alloy, and the mechanical property of steel is more stable, can become the equivalent product of now widely used VN alloy completely.In addition, adopt the ferrovanadium nitride production line of this technology foundation compared with VN alloy production line, floor space is little, energy-conserving and environment-protective, and construction speed is faster.The sales volume of the part ferrovanadium nitride that at present inventor has produced, has accounted for 50% left and right of domestic like product.
China's vanadium product can meet the demand of domestic market substantially, but the vanadium iron product that domestic metallurgical industry is used is taking 50 vanadium iron as main, the production of high vanadium ferroalloy and application percentage are very low, and in the world more uses be 70-80 VN alloy or high vanadium ferroalloy, so also just require to step up to manufacture experimently the ferrovanadium nitride of the better high vanadium of performance, promote steel products structural adjustment and upgrading to meet China.
In ZL200820126490.X patent, a kind of high pressure synthesis equipment for combustion synthesis is disclosed, it includes high pressure cylinder body, high pressure cylinder body has watercooling jacket, it is characterized in that: the scope of the internal diameter of this high pressure cylinder body is 300mm to 350mm, the scope of length is 1350mm to 1500mm, and the scope of volume is 85 liter to 150 liters; This high pressure cylinder body is one end sealing the other end hatch frame, and this high pressure cylinder body is by an end cover structure screw thread rotation means of press seals, and the sealing of the opening of this end cover structure and high pressure cylinder body seals by equal altitudes translation.This equipment can be by burning synthesis for preparing for nitrogenous 80 vanadium iron and 50 ferrovanadium nitrides.
In ZL200410057280.6 patent, the production method of a kind of burning synthesis for preparing for nitrogenous 80 vanadium iron disclosed, the method adopts combustion synthesis process or Self-propagating High-temperature Synthesis Process to prepare nitrogenous 80 vanadium iron, in nitrogenous vanadium iron, content of vanadium is 70 ± 2%, nitrogen content is 10-14%, synthetic furnace charge is that its proportioning is 80 vanadium iron 80-90% taking 80 vanadium iron and inert diluent as raw material, and inert diluent is 10-20%.
The synthetic infiltration combustion system that belongs to of nitrogenize of vanadium iron, infiltration burning is that gas-permeable enters the exothermic chemical transformation and the structural transformation process that in how empty medium, occur.In the preparation method of ZL200410057280.6 patent, we find to burn in synthetic process at 80 vanadium iron, have occurred vanadium metal molten bath because heat is too high, and metal pool also becomes a barrier that stops nitrogen infiltration, has affected nitriding effect.Secondly the passage that stops up large-area gas because of the capillary action of liquid metal, this is also unfavorable to nitrogenize building-up reactions, and therefore the top priority of high vanadium ferroalloy in the time that nitrogenize is synthetic is to reduce Synthesized temperature.The method that reduces Synthesized temperature has two kinds, and the one, the input amount of reduction unit volume internal heat generation material, the 2nd, reduce the synthetic speed of burning, reduce the thermal value in the unit time.In the time that 80 vanadium iron burnings of ZL200410057280.6 patent are synthetic, with addition of the inert diluent that has entered 15-20% to reduce synthesis temperature.But this has brought many disadvantageous effects to production, for example, the production of inert diluent makes synthesis procedure become complicated, in production, the factors of instability increase, production cost also improves thereupon, secondly, and owing to adding a large amount of thinners that the production efficiency of every heat is declined.
Therefore,, in the invention of FeV65N3 ferrovanadium nitride, we have taked a more novel short-cut method to reduce synthesis temperature, have formed the new synthetic method of a high nitrogen ferrovanadium nitride.
Summary of the invention
The inventor, on himself previous patent ZL200410057280.6 basis, adopts combustion synthesis process, produces a kind of new FeV65N13 ferrovanadium nitride product, it consists of: in quality %, V=63.0-67.0%, N=12.0-16.0%, surplus is iron and a small amount of impurity.
This FeV65N13 ferrovanadium nitride can be used as the vanadium alloy additive of Hi-Stren steel, tool steel, steel alloy or cast steel etc., and it is apparent is compact mass thing.
The inventor provides a kind of processing method of simplifying applicable production FeV65N13 ferrovanadium nitride for this reason, to ensure the synthetic smoothly of product.The raw material of FeV65N13 ferrovanadium nitride is 80 vanadium iron and 50 vanadium iron, before synthetic, 80 vanadium iron and 50 vanadium iron are respectively undertaken just mixed by 5～10 tons of quantities of goods produced, also can 50 vanadium iron be broken into Powdered, granularity is that 40-100 order is 25～40%, 100-200 order is that 25～40%, >, 200 orders are 40～55%; 80 vanadium iron are broken under protection of inert gas Powdered, granularity is that 40-100 order is that 35～50%, 100-200 order is that 40～55%, >, 200 orders are 15～30%.Vanadium iron synthesis material is after evenly mixing, be bulked in crucible, again crucible is placed in high pressure synthetic furnace, calculate institute's nitrogen requirement according to the amount of vanadium iron synthetic material, be filled with 7-12MPa high pure nitrogen and by the portfire building-up reactions of igniting, combustion synthesis reaction is complete from continuing to carry out, and no longer demand is from external complement heat energy during this time, and burning sintetics is cooling in nitrogen, be crushed to the lumpiness that user requires after coming out of the stove.
Crucible described above preferably can change plumbago crucible into, can ensure higher temperature of reaction and reduce impurity.
In the method, in raw material, the amount of 80 vanadium iron can be 80-90% weight, and the amount of 50 vanadium iron can be 10-20% weight.
In addition, can adjust vanadium iron raw material Intake Quantity according to burning synthesis device volumetric quantity and the synthetic heat producing of material combusting, when guarantee burning is synthetic there is not metal melting layer in product.
In addition, carrying out in process of combustion synthesis reaction, when nitrogen drops in burning synthetic furnace is while being low to moderate 6.5MPa, can be by one or many arbitrary way to ftercompction in burning synthetic furnace, keep nitrogen to be pressed in 7-12MPa, to meet the demand of combustion synthesis reaction to nitrogen.
For obtaining in the process of technique scheme, the inventor has carried out a large amount of tests around following many aspects.
One, reduces and participates in the inert diluent that the synthetic vanadium iron material quantity of burning replaces former ZL200410057280.6 patent interpolation.
We are in the burning synthetic furnace that packs 30-60 kilogram of ferrovanadium dust furnace charge into, reduce raw material input amount 10-25%, to replace the inert diluent amount of 15-18%, front and back have been tested 100 stoves altogether, but its effect is also unsatisfactory, still occurs melting metal layer in sintetics.Analytical data shows, the content of vanadium in metal level is 69.54%, and nitrogen content is 12.83%.In synthetic good position, content of vanadium is 68.90%, and nitrogen content is 15.16%, and content of vanadium is 68.74% in mixing zone, and nitrogen content is 14.82%.The inventor thiss is presumably because that the thermal capacity of inert diluent is large, in the process of heating by ignition, siphons away a lot of heats, although the vanadium iron synthetic material dropping in this test reduces, actual temperature of combustion does not drop to position.According to document announcement, the thermal capacity of iron is 24.958J/ ㎏ .K, and the thermal capacity of vanadium is 24.894J/ ㎏ .K, and vanadium nitride is 37.978, needs to increase 1.52 times, if continue to reduce the synthetic material dropping into, will have influence on the production efficiency of stove.
Its two, increase the particle size of 80 vanadium iron, reduce rate of combustion to reach the object that reduces Synthesized temperature.
In test design, we to the target of the synthetic FeV65N13 ferrovanadium nitride that burns are: 1. its composition should approach with former nitrogenous 80 vanadium iron; 2. do not reduce the productivity of product; 3. burn production technique synthetic and simplify, reliable, production cost is than the synthetic further reduction of former 80 nitrogenous vanadium iron; 4. in sintetics, eliminate melting metal layer; 5. vanadium and nitrogen ingredient stability in product.
In synthetic batching, adopt 50 vanadium iron and two kinds of vanadium iron of 80 vanadium iron to replace 80 single vanadium iron, to reduce heat output.And adopt multiple aggregate measures to achieve the above object.
We know, 50 vanadium iron are only itself synthetic required enough of liberated heat in the time that burning is synthetic, come deposite metal without unnecessary heat, there will not be metal melting layer, therefore, first we in vanadium iron raw material with addition of 10～20% 50 vanadium iron, to substitute the thinner of former 80 nitrogenous vanadium iron; Secondly, increase the size of 80 vanadium iron, reduce rate of combustion to reach the object that reduces Synthesized temperature; The 3rd, reduce the size of 50 vanadium iron, to maintain normally carrying out of combustion synthesis reaction; The 4th, according to the suitably Intake Quantity of the every stove raw material of adjustment of the height of the synthetic heat of burning.The object that above novelty is attempted is to ensure that whole combustion synthesis reaction carries out at lower temperature, and realizes the target setting of the synthetic FeV65N13 ferrovanadium nitride of burning.
Through conscientiously research with lot of experiments after, the inventor determines that the vanadium iron raw material of FeV65N13 ferrovanadium nitride new alloy is made up of 50 vanadium iron (FeV50) of 10-20% and 80 vanadium iron (FeV80) of 80-90%, at the beginning of 80 vanadium iron and 50 vanadium iron respectively being undertaken by 5～10 tons of quantities of goods produced (also can by the batch of user's requirement) before synthetic, mix, broken, wherein 50 vanadium iron are crushed to: 40-100 order is 25～40%, 100-200 order is that 25～40%, >, 200 orders are 40～55%; 80 vanadium iron are crushed to: 40-100 order is that 35～50%, 100-200 order is that 40～55%, >, 200 orders are 15～30%.And in former 80 nitrogenous vanadium iron, the granularity of 80 vanadium iron is: > 100 order granularities are < 10%, 100-200 order granularity is 40-50%, and >200 order granularity is 40-50%.Two kinds of vanadium iron raw material powders are after evenly mixing, be bulked in plumbago crucible, then plumbago crucible is placed in to high pressure synthetic furnace, and be filled with 7-12MPa high pure nitrogen, adopt the ignite building-up reactions of vanadium iron synthetic material one end of portfire, supplementary without external thermal source in the situation that, nitrogenize building-up reactions is from continuing to go on, until nitrogenize is synthetic complete.But nitrogen drops in synthetic furnace, to 6.5Mpa, press its nitrogen to supplementary nitrogen in burning synthetic furnace and remain on 7.0-12.0Mpa, the rate of permeation of synthesizing the demand to nitrogen and improving nitrogen to meet burning when burning.After nitrogenize has been synthesized, ferrovanadium nitride finished product is cooling and be crushed to the required block size of user in nitrogen.
To have synthesized hundreds of heats under test conditions mentioned above, the burning of FeV65N13 ferrovanadium nitride new alloy is synthetic to be carried out very wellly, can't see metal melting layer in sintetics.Owing to not containing inert diluent in synthetic material, production process is simplified, and the stability of product increases, and its production cost is also declined.
Compared with prior art, the present invention has obtained remarkable technique effect:
(1) the vanadium iron product that domestic metallurgical industry is used is taking 50 vanadium iron as main, production and the application percentage of high vanadium ferroalloy are lower, more uses is 70-80 VN alloy or high vanadium ferroalloy in the world, and the invention of FeV65N13 ferrovanadium nitride has met domestic correspondent and use the demand of the high nitrogen-vanadium alloy of high vanadium.
(2) in FeV65N13 ferrovanadium nitride new alloy synthetic owing to having cancelled adding of inert diluent, removed from and manufactured the trouble of thinner and greatly reduced process cost.
(3) in FeV65N13 ferrovanadium nitride new alloy owing to having added 50 a small amount of vanadium iron, not only suitably reduce Synthesized temperature, improve the productivity of every heat, the more important thing is that making to be difficult to 80 broken vanadium iron can have larger particle size, abrasive material time shorten, the chance that has reduced the oxidation of vanadium iron raw material, has also reduced abrasive material cost.
Specific embodiments
The concrete steps of FeV65N13 alloy embodiment are as follows: synthetic material is made up of 50 vanadium iron and 80 vanadium iron, and in batching, 50 vanadium iron account for 10-20%, and 80 vanadium iron account for 80-90%.Before synthetic by 80 vanadium iron and 50 vanadium iron respectively by 5～10 tons of quantities of goods produced carry out just mixing, broken, raw material granularity consists of: the granularity 40-100 order of 50 vanadium iron is that 25～40%, 100-200 order is that 25～40%, >, 200 orders are 40～55%; 80 vanadium iron granularities are that 40-100 order is that 35～50%, 100-200 order is that 40～55%, >, 200 orders are 15～30%.
Two kinds of vanadium iron raw material powders are after evenly mixing, be bulked in plumbago crucible, then plumbago crucible is placed in to high pressure synthetic furnace, and be filled with 7-12MPa high pure nitrogen, adopt the ignite building-up reactions of vanadium iron synthetic material one end of portfire, supplementary without external thermal source in the situation that, nitrogenize building-up reactions is from continuing to go on, until nitrogenize is synthetic complete.But nitrogen drops in synthetic furnace, to 6.5Mpa, press its nitrogen to supplementary nitrogen in burning synthetic furnace and remain on 7.0-12.0Mpa, the rate of permeation of synthesizing the demand to nitrogen and improving nitrogen to meet burning when burning.After nitrogenize has been synthesized, ferrovanadium nitride finished product is cooling and be crushed to the required block size of user in nitrogen.
According to above-mentioned synthetic method, and burn and synthesize FeV65N13 ferrovanadium nitride embodiment 1-15 according to the synthetic parameters providing in following table 1.
The embodiment of the synthetic FeV65N13 ferrovanadium nitride of table 1 burning
Data by table 1 can obviously find out, the 1st example causes burning because granularity is meticulous, and synthetic heat is too high occurs that metal melting layer is more, and nitrogen content is on the low side, and synthetic finished product is defective; The 2nd example is crossed and is slightly caused burning the synthetic too low synthetic failure of heat because of granularity; Other 13 routine combustion synthesis reaction carries out smoothly at lower temperature, and the ferrovanadium nitride product composition fluctuation of different embodiment corresponding each batch is very little, shows that quality product of the present invention is more stable, and production technique is reliable.In addition simple, the cost of the inventive method synthesis technique.
This written description use-case discloses the present invention, comprises optimal mode, and also makes those skilled in the art can manufacture and use the present invention.Scope that can granted patent of the present invention is defined by the claims, and can comprise other example that those skilled in the art expect.If this other example has the structural element of the literal language that does not differ from claims, if or this other example comprises and the literal language of claims equivalent structure element without substantial differences, within this other example is intended to the scope in claims.Can not cause under inconsistent degree, by reference to all references part of reference is herein incorporated herein.
Claims (8)
1. a FeV65N13 ferrovanadium nitride, it consists of: in quality %, V=63.0-67.0%, N=12.0-16.0%, surplus is iron and a small amount of impurity.
2. according to the ferrovanadium nitride of claims 1, wherein said FeV65N13 ferrovanadium nitride is as the vanadium alloy additive of Hi-Stren steel, tool steel, steel alloy or cast steel etc.
3. according to the ferrovanadium nitride of claims 1 or 2, it is compact mass thing.
One kind by burning synthesis for preparing the method for ferrovanadium nitride described in claims 1, its raw material is 80 vanadium iron (FeV80) of 80-90% weight ratio and 50 vanadium iron (FeV50) of 10-20% weight ratio, before synthetic, 80 vanadium iron and 50 vanadium iron are carried out just mixed, 50 vanadium iron are broken into Powdered, 80 vanadium iron are broken into Powdered under protection of inert gas, vanadium iron synthetic material is after evenly mixing, be bulked in crucible, again crucible is placed in high pressure synthetic furnace, be filled with 7-12MPa high pure nitrogen and by the portfire building-up reactions of igniting, finished product after having reacted is cooling in nitrogen, come out of the stove, be crushed to user's desired particle size.
5. prepare as claimed in claim 4 the method for ferrovanadium nitride, it is characterized in that described crucible is plumbago crucible.
6. prepare as claimed in claim 4 the method for ferrovanadium nitride, it is characterized in that, it is that 40-100 order is 25～40% that described 50 vanadium iron are crushed to granularity, 100-200 order is 25～40%, > 200 orders are 40～55%(weight ratio), it is that 40-100 order is that 35～50%, 100-200 order is that 40～55%, >, 200 orders are 15～30%(weight ratio that described 80 vanadium iron are crushed to granularity).
7. prepare according to claim 4 the method for ferrovanadium nitride, carrying out in process of combustion synthesis reaction, in the time that in burning synthetic furnace, nitrogen drops is low to moderate 6.5MPa, press one or many supplement nitrogen mode to burning synthetic furnace in ftercompction, keep nitrogen to be pressed in 7-12MPa, make to meet the demand of combustion synthesis reaction to nitrogen.
8. according to the method for claim 5, adjust vanadium iron raw material Intake Quantity according to burning synthesis device volume and the synthetic heat producing of vanadium iron material combusting, to ensure to burn there is not metal melting layer in synthetic product.
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| CN104593632A (en) * | 2015-01-23 | 2015-05-06 | 武钢集团昆明钢铁股份有限公司 | Preparation method of nitriding ferrocolumbium alloy |
| CN107457407A (en) * | 2017-07-21 | 2017-12-12 | 湖南众鑫新材料科技股份有限公司 | A kind of breaking method of ferrovanadium nitride |
| CN107904425A (en) * | 2017-11-27 | 2018-04-13 | 攀钢集团钒钛资源股份有限公司 | The preparation method of ferrovanadium nitride |
| CN110875110A (en) * | 2018-08-29 | 2020-03-10 | 射洪福临磁材有限公司 | VN particle-containing neodymium iron boron magnetic material and preparation method thereof |
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| CN110875110A (en) * | 2018-08-29 | 2020-03-10 | 射洪福临磁材有限公司 | VN particle-containing neodymium iron boron magnetic material and preparation method thereof |
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